Month: February 2021

Application of 351003-36-6, These common heterocyclic compound, 351003-36-6, name is 2-Fluoro-5-iodobenzonitrile, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a stirred solution of terf-butyl frans-4-(4-chlorophenyl)-3- (hydroxymethyl)piperidine-l-carboxylate (2.20 g, 6.75 mmol) in anhydrous N,N- dimethylformamide (100 mL) was added sodium hydride (0.35 g, 8.8 mmol, 60% w/w dispersion in mineral oil) at 0 C. The reaction mixture was stirred at ambient temperature for 30 minutes. 2-Fluoro-5-iodobenzonitrile (1.83 g, 7.40 mmol) was added at 0 C and the reaction mixture was stirred at ambient temperature for 16 h. Saturated ammonium chloride (50 mL) was added, followed by ethyl acetate (200 mL). The organic layer was washed with brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo. The residue was purified by column chromatography (5%-50% gradient of ethyl acetate in hexanes) to afford iert-butyl irans-4-(4-chlorophenyl)-3-((2-cyano-4-iodophenoxy)methyl)piperidine-1-carboxylate in 88% yield (3.30 g) as a colorless solid: MS (ES+) m/z 552.8 (M + 1), 554.8 (M + 1).

The synthetic route of 351003-36-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; XENON PHARMACEUTICALS INC.; SUN, Shaoyi; ZENOVA, Alla, Yurevna; CHAFEEV, Mikhail; JIA, Qi; ZHANG, Zaihui; OBALLA, Renata, Marcella; WO2013/64983; (2013); A1;,
Iodide – Wikipedia,
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Synthetic Route of 111771-08-5, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 111771-08-5, name is 2-Fluoro-6-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

Intermediate 14: 2-Fluoro-6-pyrimidin-2-yl-benzoic acid.Step A: 2-Fluoro-6-iodo-benzoic acid methyl ester. To a 200 mL round- bottomed flask were added 2-fluoro-6-iodo-benzoic acid (7.5 g, 28.2 mmol), LiOH?H20 (1 .42 g, 33.8 mmol), and THF (100 mL). The resulting mixture was warmed to 50 C and stirred for 2 h. Dimethyl sulfate (4.03 mL, 42.3 mmol) was then added and the mixture was warmed to 65 C. After 2 h, the mixture was cooled to room temperature and NH4CI(ag) (50 mL, 13 wt% solution) was added. The two resulting layers were thoroughly mixed and then separated. The organic layer was dried over MgS04, filtered, and concentrated under reduced pressure to a light brown oil (7.79 g, 99% yield). 1 H NMR (400 MHz, CDCI3): 7.68 – 7.60 (m, 1 H), 7.15 – 7.06 (m, 2H), 3.98 (s, 3H).

The chemical industry reduces the impact on the environment during synthesis 2-Fluoro-6-iodobenzoic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; LETAVIC, Michael; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHIREMAN, Brock, T.; SWANSON, Devin; WO2012/145581; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Safety of 1,2-Dichloro-3-iodobenzene

D. 17alpha-Chloro-17beta-Methylsulfinyl-1,4-Androstadiene-3,11-Dione In a manner similar to that described in Example 2A, react 2.4 gm. of 17alpha-methylthio-1,4-androstadiene-3,11-dione, 55.6 ml. of pyridine, 14.4 ml. of water and 5.76 gm. of iodobenzene dichloride. Pass the concentrated residue through a 250 gm. silica gel column, eluding first with chloroform and then with ethyl acetate. Evaporate the ethyl acetate eluates and crystallize from acetone/hexane to obtain the title compound; nmr (CDCl3) delta 1.21 (C13 –CH3, s), 1.45 (C10 –CH3, s), 2.55 (S–CH3, s), 6.10 (C4 –H, d), 6.20 (C2 –H, dd), 7.68 (C1 –H, d).

The synthetic route of 1,2-Dichloro-3-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Schering Corporation; US4183924; (1980); A;,
Iodide – Wikipedia,
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Synthetic Route of 54413-93-3, The chemical industry reduces the impact on the environment during synthesis 54413-93-3, name is 2-Iodo-5-methoxybenzoic acid, I believe this compound will play a more active role in future production and life.

General procedure: In a 10 mL glass tube 2-iodobenzoic acid (1.0 mmol), acetamidine hydrochloride (1.2 mmol), CuCl2 (0.1 mmol), L2 (0.1 mmol), and NaOH (4.0 equiv.) and 3.0 mL water were placed. The vessel was then sealed with a septum and placed into the microwave cavity. Initial microwave irradiation of 120 W by using a CEM Discover microwave synthesizer was used at the room temperature for 20 min. The reaction mixture was stirred continuously during the reaction. After completion of the reaction, the solvent was removed in vacuo. The residue was purified by silica gel column chromatography to afford the corresponding product. All the products were confirmed by NMR and MS spectroscopic analysis.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Iodo-5-methoxybenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ke, Fang; Liu, Caiqin; Zhang, Peng; Xu, Jianhua; Chen, Xiaole; Synthetic Communications; vol. 48; 24; (2018); p. 3089 – 3098;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 88-67-5, name is 2-Iodobenzoic acid, molecular formula is C7H5IO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Application In Synthesis of 2-Iodobenzoic acid

2.48 g (10 mmol) of o-iodobenzoic acid was weighed, and 5 mL of absolute ethanol was weighed. Magnetic seeds were placed in a round bottom flask, and an appropriate amount of concentrated sulfuric acid was added thereto, and the mixture was stirred at 90 C for 12 hours, and detected by TLC, and stopped when the raw materials disappeared. reaction. The reaction solution was concentrated by a reduced pressure rotary evaporator to remove excess ethanol, and an appropriate amount of saturated NaHCO 3 was added to neutralize the remaining concentrated sulfuric acid.When no bubbles are generated, that is, when the neutralization is complete, the mixture is washed with ethyl acetate (3¡Á50 mL) and water, and the organic layer is combined, water is evaporated, and filtered, and then filtered, and then filtered, and then evaporated. The ethyl acetate was removed to give 2.50 g of ethyl iodobenzoate as a yellow oil, yield 90%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 88-67-5, its application will become more common.

Reference:
Patent; Xinxiang Medical University; Xinxiang Medical School San Quan College; Yan Fulin; Wang Yawen; Yan Jianwei; Yin Tiantian; Ma Jinshuo; (15 pag.)CN110183387; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 103962-05-6, These common heterocyclic compound, 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a solution of 1-iodo-4-(trifluoromethoxy)benzene (288 mg, 1.0 mmol) and 6-chloro-5-methylpyridin-3-ylboronic acid (223 mg, 1.3 mmol) in DMF (2 mL) was added K2CO3 (552 mg, 4.0 mmol) and H2O (0.5 mL). The reaction mixture was stirred for 5 min under an atmosphere of dry N2. Pd(PPh3)4 (10 mg, 0.009 mmol) was added, and the resulting mixture was subjected to irradiation at 120¡ã C. for 10 min. Cooled, diluted with EtOAc (20 mL), filtered through a layer of celite, washed with 10percent DMF in EtOAc (50 mL), transferred to a separation funnel, organic phase was washed with 2N Na2CO3 (20 mL, 4.00 mmol), H2O (20 mL), 30percent aqueous NH4Cl (50 mL) and brine (50 mL), and dried and concentrated. The crude mixture was subjected to preparative HPLC with a gradient MeCN/H2O (5percent to 98percent) containing 0.1percent TFA to afford 2-chloro-3-methyl-5-(4-(trifluoromethoxy)phenyl)pyridine,MS m/z 288.0 (M+H), HPLC purity>97percent.

The synthetic route of 103962-05-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Gilead Palo Alto, Inc.; US2011/21521; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 610-97-9, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 610-97-9, name is Methyl 2-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Methyl 2-iodobenzoate (25 g, 95 mmol), prop-2-yn-1-ol (8.02 g, 143 mmol) and TEA (26.6 ml, 191 mmol) were added to a deareated mixture of Pd(PPh3)4 (0.220 g, 0.191 mmol), copper(I) iodide (0.073 g, 0.382 mmol) in DMF (60 ml). The resulting mixture was stirred at 90 C. for 5 hrs and then at 40 C. overnight. The reaction mixture was poured into EtOAc (600 ml) and washed with brine (600 ml). Organic phase was then concentrated and the dark oil was rinsed with Et2O (600 ml). The mixture was filtered, and then concentrated to give the title compound as deeply brown oil (13.0 g). This compound was used in the next step without any further purification and characterization. UPLC-MS: 1.53 min, [M+H-18]+. (Method 4)

The synthetic route of Methyl 2-iodobenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHIESI FARMACEUTICI S.p.A.; Biagetti, Matteo; Capelli, Anna Maria; Accetta, Alessandro; Carzaniga, Laura; US2015/166549; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 101335-11-9, The chemical industry reduces the impact on the environment during synthesis 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, I believe this compound will play a more active role in future production and life.

Sodium methanethiolate (5g) was added to a solution of 4-fluoro-2-chloro-iodobenzene (18.3g) and stirred for 20h. The mixture was poured into water, extracted with ether, washed with brine, dried (MgS04) and evaporated. Yield 18. 5g. 1H NMR DMSO-d6: 8 7.81 (d, 1H), 7.43 (dd, 1H), 6.98 (dd, 1H), 3.32 (s, 3H)

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Chloro-4-fluoro-1-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; WO2004/89885; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 1-Iodo-2-(trifluoromethyl)benzene

General procedure: 9-[2-(4-Nitrophenoxy)naphthalene-1-yl]-11,12-dihydro-10H-indeno[6,5,4-kl]xanthene (3a): A mixture of 1a (73.6 mg, 189 mumol, 1.00 equiv.), 2 (67.1 mg, 198 mumol, 1.05 equiv.), Pd(OAc)2 (4.22 mg, 18.8 mumol, 0.10 equiv.), PPh3 (24.7 mg, 94.0 mumol, 0.50 equiv.) and (nBu)4NOAc (341 mg, 1.13 mmol, 6.00 equiv.) in degassed DMF (5 mL) was stirred at 100 ¡ãC for 21 h. The reaction mixturewas filtered through SiO2, flushed with EtOAc and the solvent of the filtrate was removed in vacuo.Column chromatography (SiO2, n-pentane/EtOAc 20:1) yielded 3

The synthetic route of 1-Iodo-2-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tietze, Lutz F.; Eichhorst, Christoph; Heterocycles; vol. 90; 2; (2015); p. 919 – 927;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 69113-59-3, name is 3-Iodobenzonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 3-Iodobenzonitrile

General procedure: Aryl-halide (0.2 mmol, 1 equiv.), Ir(dtbbpy)(ppy)2PF6 (1.8 mg, 0.002 mmol, 1 mol %), NiCl2.glyme (4.4mg, 0.02 mmol, 10 mol %), DMSO (2.0 mL) was added to a 10 mL schlenk flask equipped with a magnetic stirrer bar. This resulting mixture was sealed and degassed via vacuum evacuation and subsequent backfill with ethylene for three times. Then, N,N,N?,N?-tetramethylethylenediamine, TMEDA(60 muL, 2 equiv.), N,N-diisopropylethylamine, DIPEA (70 muL, 2 equiv.) and H2O (7.2 muL, 2 equiv.) were subsequently added in this order. The mixture was then irradiated with blue LED (2 meter strip, 18 W)with ethylene balloon for 24 hours at 80oC (Figure S1). The reaction was added water (30 mL) and extracted with ethyl acetate (10 mL) three times. Combined organic layer was successively washed with brine three times and dried over Na2SO4 and concentrated under reduced pressure. The residue was then subjected to flash column chromatography (hexane or hexane/ethyl acetate) to yield theproduct

The synthetic route of 69113-59-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Jiesheng; Luo, Yixin; Cheo, Han Wen; Lan, Yu; Wu, Jie; Chem; vol. 5; 1; (2019); p. 192 – 203;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com